Process for obtaining cyanogen and its compounds.



J. BUEB. PROCESS FOR OBTAINING CYANOGEN AND ITS COMPOUNDS.

APPLIOATION FILED OUT. 1910 I I -latented Jul-y 16, 1912.

JULIUS BUEB, OF DESSAU, GERMANY.

PROCESS FOR OBTAINING cYANoGEn; AND ITS COMPOUNDS.

Specification of Letters latent.

Patented July 16, 1912.

Application filed Octdber 26, 1910. Serial No. 589,257.

To all whom it may concern:

Be it known that I, JULIUS BUEB, a subject of the German Emperor, and resident of Dessau, Germany, have invented certain new and useful Improvements in Processes for Obtaining Cyanogen and its Compounds, of which the following is a specification.

My invention relates to the utilization of the distillation products of distillers waste, and has for its objectto obtain from them cyanogen and cyanogen compounds.

In processes hitherto known, the gases resulting from the distillation of distillers waste are heated to such a high temperature that the substances therein which can be cyanized are converted into cyanogen compounds, but in such processes a large quantity of indifierent substances, not capable of conversion into cyanogen compounds, and of steam exceeding in amount the substances capable of being converted into cyanogen compounds, are' heated with the latter to the required high temperature necessitating a large expenditure of t'uel. These non-cyanizable substances dilute those that are cyanizable to such an extentthat a part of the latter escape the cyanizing action while being heated and leave the h ating apparatus without being converted into cyanogen compounds, so that only a low yield is ob .tained.

The object of the present invention is to overcome the above noted objections and it provides 'for treating the gases and vapors from distillcrs waste to separate therefrom the substances which cannot be converted into cyanid compounds before said gases and vapors are superheated to form cyanogen compounds.

The accompanying drawing illustrates, more or'lcss conventionally, one form of apparatus adapted for carrying ,out the process hereinafter more particularly described.- g k The apparatus illustrated comprises a carboniuing furnace 1 with a retort 2 having a suitable inlet and outlet. The retort outlet is connected by a pipe 3 with a'eoudcnscr 4, preferably operated with water A pipe 5 connects the lower portion of the condenser with the lower portion of a scrubber 6 and a brangh {of said pipe leads to the upper portion of the scrubber whichzlatter 18 providcd at its a jper end with a gas outlet 8. The scrubber is conne ted through a pipe 9 with a distilling column 10 and a pipe 11 leads from the latter to a cyanizing heater 12 which is provided with a gas outlet 13.

In carrying out the. invention tin-gases and vapor-like products passing otl from the-outlet 2 during the carbonization process at a temperature of from IOO JOU C.

are conveyed through pipe 3 into the condenser 4. Thiscondenscr is cooled with wa ter whereby the temperature of the. gaseous substances is reduced to that of the atmosphere and part of them are liquefied. The

condensate carries only a part of the nitro! gen compounds capable of conversion into cyanogen-compounds, the greater part still existing in gaseous form, which is recovered, however, by conducting the gas through pipe 5 into the scrubber 6 anclthere washing it with the condensatementioned above which is conducted to the to) of the scrubber by the pipe 7. This wasliing process is carried out on the principle of the countercurrent. In this way all the constituents of the gases, which are cyanizable are taken up by the condensate which is thereby'enrichcd while the components whichare not capable of being coudensed,'because they are insoluble in the condensate, escape in the gaseous form through outlet8 and are, as theyare combustible, utilized for heating the carbonizing furnace, or for other heating purposes. The condensate which is rich in nitrogen, is conducted through pipe 9 to column 10 where it is subjected to a distilling process at a temperature which lies below the boiling point of the liquor, wherebyis obtained a distillate of compounds, which is now free from water and substances incapable of conversion into cyanogen compounds, and this is then supplied to the cyanizing heaters 1'2. Thecyanization of the'distillation products is carried on at a temperature of about 1,000 C. and owing to the hereinbefore described removal of non-cyanizable substances, the process is carried oneasily and perfectly, the cyanogen gases thus obtained, and composed to a large extent of hydrocyanic' aci lealing 1 the heater 12 through the outlet 13 and ma be subsequently absorbed and t-ransforme into alkali-cyanid in the way well known There is also the advantage, that the gases supplied to the cya'nizmg in the art.

heater are free from substances which b e come carbonized at the high heating tern perature and thus mightobstruct the fines;

these substances are not however wasted since, asfal'ready mentionedp they; can: be used for heating urposes, The teohni'cal and, economical" a vantages of: the; present" 1 process are obvious to every expertin the art; r

ounds are; met-hylhnx ifi} dis methyemin, trxmethylannnand higher homol'ognes, ammonium carbonate and some jiitrog'enousrbodies of unknown constitution. 1 :The sepsration of trimethylamin from the 'k'asesofthe distillers waste andiits subsejqnent'cyanization have, already. been deseribed' in technical literature. V Owing, how.-

ever tothe factthat thesaid gases contain, -bes1de's -trinlethylmnin,v other substances ce- Pablo of oon'version, into cyanogen compounds; thisisolation of the trimethyleminalone {proved unsatisfactory from technical and'eeonomioal points of, view, so that the process was soon oiseaz'ded innthis industry.

- Aflgce'at sq-vantage of the present process 13 that the'yield ot eyenogen-compoundsis aperfect. one, for-no losses are :sustainedkby. the operations of depriving the gases of the =cyan1zab1e compounds as well as by distillm these compounds from the highly enric ed washingfluid. Thehereinbeforedeseribediproc'ess fonthe treetmentof the gases (from the carbonization ofglistillers' waste.

eannlso'v be-applied wherever gases and vapprs .canbe dealt with'whioh consist partly of cyanizable, ,and partly of mm cyanizable substances. s

4-5 vcntionally one form of "apparatus adapted It will of course be-understood that the invention -is not limited-t0 the use'ofany particular apparatus and may be carried out with parts constructed and arranged very 'difierentfrom those illustrated, the illustrw tion being furnished meply to show eonfor carrying out the process. 4

Having'thus described the inventionpvhat isc1aimedis: I I 1. The hIerein-de'crib'od improvement in" theprocess of 'xnenuqncturing cyanogen com- BEST AVAILABLE COPY pounds from the gases and vapors produced during the earbomz'atlon or" nitrogenous substances, such as. distillers waste,v comprising separatinfiseid sees and vapors into their' cyaniza e an non=cyanizable constituents, and lgthen treatingithe cyanizable A constituents to efiecU-transformation thereof into cyanogen compounds.

2.i'1 h1e hereingdescribed improvement in the'process'of manufacturing cyanogen compounds from'the gases'and apors produced durmg'the earbomzation' or nitrogenous substances, sueh as distillers'waste, comprising;

separating said gsses md vapors into their cyaniza'blel and' non-"cyamzable constituents by cooling the, same and then ti'eating the cyanizable constitnel'its to effect ti'ansfotina tion .-thereof'into cyanogen compounds."

3; The herein-described improvement in the process of manufacturing cyanogen-compounds. from the gases and Ivapors produced during-the carbonization of nitrogenous sub stnnces,'.such' usjdist iliers wa te, comprising j cooling said gases and vapors toliqnefy "s'u ch as are 'cmnlensnble ;washing the gases and vapors with the condensate obtained by'sxjuph cooling operation, and. thentyeating the-- cvnniimhle ases to. effect tmnsforma{ion D I r "i heaeof into cyanogen compounds.

4; The herein-descrioed pi ocess of menu '80 fnctm'ing cyanogen compounds" from the" gases and vapors prod-need during thecarbonlzfitxon of nitrogenous sidostzmces, such 1 as distillers waste, consisting in coolingsnidgases and vapors-to liqnefy snch/z'is'm'o 0on densable, washing the gases and Vapors with the condensateiobtained by the cooling op eration, liberating the nit'hbge'nous' su st ances' contained in the washing flnid and then treating the cyaniznhi gases to effect thereof into cyanogen oom 7 transfornmtionpounds.

1 In testimony"wh'reof'ii have signed-my name to flus specxficahon i-n' the presence of y t h .hvosubscribing'witnessesl i \Vitness'es Renown:1 11163311, lg 

